Preparation containing colloidal compounds.



CARL PAAL,

SIGNORS TO THE FIRM OF KALI E 86 BIEBRICH, GERMANY.

OF LEIPZIG, AND CONRAD AMBERGER, 0F ERLANGEN, GERMANY, AS-

COMI'ANY, AKTIENGESELLSCHAFT, OF

PREPARATION CONTAINING COLLOIDAL COMPOUNDS.

Patented Nov. 4, 1913.

No Drawing. Original application filed May 12, 1913, Serial No. 767,205.Divided and this application filed September 27, 1913. Serial No.792,177;

T 0 all whom, it may concern:

Be it known that we, CARL PAAL, resident of Leipzig, and CONRADAMBERGER, resident of Erlangen, Germany, both citizens of the GermanEmpire, have invented certain new and useful Improvements inPreparations Containing Colloidal Compounds, of which the following is aspecification.

Inour patent specification Ser. No. 767,205, of May 12th, 1913, of whichthe present case is a division, We have described theproduction ofpreparations of a greasy consistency containing inorganic metal colloidsoffthe platinum group. This process consists in incorporating solutionsof the divalent salts of the metals of the platinum group with bodies-maintaining colloids in the colloidal state (protecting colloids)especially with wool fat or the alcohols obtainable therefrom bysaponificatiomand adding a carbonate of an alkali to form the colloidallower hydroxide of the metals em ployed. Now we have found that alsopreparations containing combinations'of the divalent salts of the metalsof the platinum group in a colloidal condition can be obtained, ifinstead of the alkali carbonates used in the above mentioned process,the alkali salts of certain weak organic acids are selected, forinstance the salts of the higher, saturated, or unsaturated, fatty acids(soaps). In this way there are produced in the presence of solutions ofthe said. metal salts for instance of the divalent palladium,

' or platinum, triturated with wool fat, products which contain thecorresponding palladium, or platinum, salts dissolved in colloidal formin the wool fat. This could not have been foreseen, because it was to beassunicd that these platinum, or palladium, salts would split off byhydrolysis with weak organic acids in the presence of the water requiredfor the solution of the components.

- The-platinum and palladium salts of fatty acids are more or lessstrongly dissociated by hydrolysis in the presence of water or aqueoussolution; more especially is this true of the fatty acids of highmolecular weight such, for instance, as palmitic, stearic, or olc cacids. On this dissociation depends, as Is well known, the act-ion ofthe ordinary washing soaps, which are" salts of the Strong bases,potash, and soda.

If, as initial materials, definite quantities of wool fat and inorganicpalladious or platinous salts be used, products having a quite definite.content of palladium, or platinum, organo'sols can be obtained.

The content of colloidal palladium and platinum compounds in thepreparations can be enriched by partially precipitating solutions of theproducts having a definite content-of palladium, or platinum, colloid,for instance the solutions in pretroleum ether, obtainable during therocess by an organic liquid in which wool at, or wool tat alcohols, aredifiicultly soluble. The surprising result is then obtained that thecorresponding colloidal platinum compounds pass quan- "titatively intothe precipitate with a part of the wool fat, whereby they fully retaintheir colloidal character, so that the precipitations which present acorresponding higher amount of the corresponding platinum metal colloid,likewise possess the valuable property of being absorbed in the form ofthe liquid organosols, by all organic liquids dissolving wool fat orwool fat alcohols.

The following example will further illus- I trate how this lnvention canbe carried into practice, but the invention is not limited -to the saidexample.

Example-Production of a preparate'on containing 25 per cent. colloidalpalladious 0leate.If wool fat be impregnated with a concentrated aqueoussolution of palladious chlorid (PdCl and the mass be then trituratedwith the equivalent quantity of potas sium 'oleate in concentratedaqueous solution, the salts mutually decompose with formationofpotassium chlorid and palladious oleate which as already statedremains dissolved incolloidal-form in the wool fat. ;As

the palladious chlorid is diificultly soluble in ure water, but readilyin hydrochloric aci it is dissolved in the latter and the acid isneutralized before triturating the liquid with wool fat by ,means of anamount of sodium carbonate equivalent to the hydrochloric acid used; Theneutral PdCl, then remains dissolved in the liquid.-

' In order to obtain a preparationcontaining about 25 per cent,colloidal palladious oleate 0.85- parts of palladious chlorid PdCl=0.5.parts of palladium are dissolved with the application of heat in0.45 parts of fuming hydrochloric acid (38 per cent. H01) and 2 parts ofwater, and the hydrochloric acid is neutralized by the addition of 0.3parts of anhydro'us soda either solid or dissolved in 0.7 parts ofwater. The solution of PdCl thus obtainedris then tritue ratedintimately in small portions with 9.5 parts of Wool tat softened at agentle heat. Into the ointment body thus obtained are then stirred, alsoin small portions, 3.5 parts of potassium oleate dissolved in 15 partsof water. The formation of the palladium oleate is detected by the factthat the greasy mass colored red-brown by thepalladious chlorid becomes,on being triturated with the potassium oleate, first yellow-brown, thengray-brown and, after being allowed to stand some'considerable time,black-brown. For the purpose to urify the product it may be eithertreated repeatedly with hot water at from 50 to 60 centigrade, and theointment mass dried in vacuo at from 4:0" to 50 centigrade, for thepurpose of removing the water; or the original product may be dissolvedin from 5 to 6 times its volume of petroleum ether of low boiling point,the greater part of the by-products remaining undissolved and thered-brown liquid organosol being dried with calcium chlorid ordehydrated sodium sulfate. In this case a further part of theby-products separates along with the water. The petroleum ether is thendistilled oil from the liquid freed from the drying agent.

The colloidal palladium oleate can be enriched in the ointment body inthe manner hereinbefore described, by dissolution in petroleum etherandprecipitation with alcohol. A product is thus obtained containingabout 70 per cent. of, colloidal palladium oleate, which like the 25 percent. preparation, is absorbed as organosol by all organic substancesdissolving wool fat.

In lieu of oleic acid, other higher fatty acids which form alkali saltssoluble in water can be used. Likewise, instead of a palladious salt aplatinous or other salt of the platinum group can be used for instancethe salt of divalent platinum resulting from the reduction of theplatino-chlorid-hydro- .chloric acid with sulfur dioxid. If under theconditions of investigation already stated, wool fat impregnated with aplatinous salt be acted on by an aqueous solution of potassium oleate, acolloidal platinousoleate (C H O Pt is formed.

Inasmuch as the wool fat acts in the present process as a bodypreserving the colloidal state of the salts of the metals of the platinogroup other mediums may be employed instead of the wool fat fulfillingthe same efi:'ect. So for instance the mixture of the wool fat alcoholsobtained from wool fat by saponification can be used in the same manner.The wool fat alcohols are in their properties very similar to the woolfat itselfand the mixture of alcohols obtained therefrom bysaponification presents a still greater aflinity for water than woolfat. The wool fat alcohols have a more solid consistency, than the woolfat. According as it is desired to obtainpreparations of harder orsofter quality, the initial material used for the purpose is either amixture of wool fat alcohols per se or their mixture with wool fat,which last mixture is obtained by melting the components together. Theproduction of the ointment preparations is effected in the describedmanner. The wool fat alcohols are accordingly considered the equivalentof the wool fat in the process and product of the present invention.

We claim:

1. Process for the production of preparations containing inorganiccolloids, consisting in incorporating a solution of a divalent salt of ametal of the platinum group with a protecting colloid, adding a soapsolution to form the colloidal soap of the metal and removing theby-products formed in the process from the resulting preparation.

2. Process for the production of preparaing in incorporating a solutionof a divalent salt of a metal of the platinum group with a protectingcolloid, adding a sea solution to form the colloidal soap, disso vingthe soft mass, mixing the solution with a liquid sparingly dissolving ornot dissolving the protecting colloid and separating the precipitatecontaining the colloid.

3. Process for the production of preparations containing inorganiccolloids, which consists in incorporating with a solutionof a divalentsalt of a metal of the platinum group wool fat as a protecting colloid,addlng an alkali salt of a higher fatty acid to form a colloidal soap ofthe metal, and removing the by-products formed in the process from theresulting preparation.

4. Process for the production of preparations containing inorganiccolloids, which consists in incorporating with a solution of a divalentsalt of a metal of the platinum group, a protecting colloid, convertingsuch metal into the form of an oleate by treating with a soluble alkalioleate, and removing the by-products formed in the process from theresulting product.

5. As new roducts preparations containing a colloi al soap of a metal ofthe platinum group together with a protecting colloid. 0

6. As new products, 1preparations containing a colloidal soap 0 adivalent metal of the platinum group, together with wool fatconstituents as a protective colloid.

7. As new products, preparations containtions containing inorganiccolloids, consist of a divalent metal of ing a colloidal soap f 9. Asnew products, preparations containing Colloidal palladious soap,together with wool fat constituents as a protective colloid.

10. As new products, preparations containing colloidal palladious soatogether with wool fat as a rotective coll oid.

11. As new pro ucts, preparations containing a colloidal oleate of adivalent metal of the platinum group, together with wool fatconstituents as a protective colloid.

12. As new products, preparations con taining a colloidal oleate of adivalent metal of the platinum group, together with wool fat as aprotective colloid.

13. As new products, preparations con taining colloidal palladiousoleate, together with a protective colloid.

14. As new products, preparations containing colloidal palladiousoleate, together with wool fat constituents, as a protective colloid.

15. As new products, preparations containing colloidal palladiousoleate, together with wool fat as a protective colloid.

In testimony whereof we have signed our names to this specification inthe presence of two subscribing witnesses.

CARL PAAL. CONRAD AMBERGER. Witnesses as to signature of Carl Paal:

MAX BEEsnN, HERMANN Arrrzun.

Witnesses as to signature. of Conrad Amberger:

OSCAR Boon,

GEORGE NICOLAS IFFT.

